Regulating the dopant clustering in LiZnAs-based diluted magnetic semiconductor

Tuning of the magnetic interaction plays the vital role in reducing the clustering of magnetic dopant in diluted magnetic semiconductors(DMS).Due to the not well understood magnetic mechanism and the interplay between different magnetic mechanisms,no efficient and universal tuning strategy is proposed at present.Here,the magnetic interactions and formation energies of isovalent-doped(Mn) and aliovalent(Cr)-doped LiZnAs are studied based on density functional theory(DFT).It is found that the dopant–dopant distance-dependent magnetic interaction is highly sensitive to the carrier concentration and carrier type and can only be explained by the interplay between two magnetic mechanisms,i.e.,superexchange and Zener’s p–d exchange model.Thus,the magnetic behavior and clustering of magnetic dopant can be tuned by the interplay between two magnetic mechanisms.The insensitivity of the tuning effect to U parameter suggests that our strategy could be universal to other DMS.

Development of 400-μW cryogen-free dilution refrigerators for quantum experiments

We have successfully developed cryogen-free dilution refrigerators with medium cooling power that can be applied to quantum experiments. Breakthroughs have been made in some key technologies and components of heat switches and dilution units. Our prototype has been running continuously and stably for more than 100 hours below 10 m K, with a minimum temperature of 7.6 m K and a cooling power of 450 μW at 100 m K. At the same time, we have also made progress in the application of dilution refrigerators, such as quantum computing, low-temperature detector, and magnet integration. These indicators and test results indicate good prospects for application in physics, astronomy, and quantum information.

Correlation of work function and stacking fault energy through Kelvin probe force microscopy and nanohardness in diluteα-magnesium

Electronic interactions of the Group 2A elements with magnesium have been studied through the dilute solid solutions in binary Mg-Ca,Mg-Sr and Mg-Ba systems.This investigation incorporated the difference in the‘Work Function'(ΔWF)measured via Kelvin Probe Force Microscopy(KPFM),as a property directly affected by interatomic bond types,i.e.the electronic structure,nanoindentation measurements,and Stacking Fault Energy values reported in the literature.It was shown that the nano-hardness of the solid-solutionα-Mg phase changed in the order of Mg-Ca>Mg-Sr>Mg-Ba.Thus,it was shown,by also considering the nano-hardness levels,that SFE of a solid-solution is closely correlated with its‘Work Function'level.Nano-hardness measurements on the eutectics andΔWF difference between eutectic phases enabled an assessment of the relative bond strength and the pertinent electronic structures of the eutectics in the three alloys.Correlation withΔWF and at least qualitative verification of those computed SFE values with some experimental measurement techniques were considered important as those computational methods are based on zero Kelvin degree,relatively simple atomic models and a number of assumptions.As asserted by this investigation,if the results of measurement techniques can be qualitatively correlated with those of the computational methods,it can be possible to evaluate the electronic structures in alloys,starting from binary systems,going to ternary and then multi-elemental systems.Our investigation has shown that such a qualitative correlation is possible.After all,the SFE values are not treated as absolute values but rather become essential in comparative investigations when assessing the influences of alloying elements at a fundamental level,that is,free electron density distributions.Our study indicated that the principles of‘electronic metallurgy'in developing multi-elemental alloy systems can be followed via practical experimental methods,i.e.ΔWF measurements using KPFM and nanoindentation.

First-Principle Study on the Electronic Structure and Optical Property of New Diluted Magnetic Semiconductor(Y_(0.75)Ca_(0.25))(Cu_(0.75)Mn_(0.25))SO

The band structure,DOSs,and optical properties of(Y_(0.75)Ca_(0.25))(Cu_(0.75)Mn_(0.25))SO,including dielectric function,absorption function,reflection function,and energy loss spectrum were studied by using the first-principles calculation.The calculation results indicate that(Y_(0.75)Ca_(0.25))(Cu_(0.75)Mn_(0.25))SO is a direct bandgap semiconductor with a bandgap of 1.1 eV.The Fermi surface is asymmetric and exhibits spin splitting phenomenon.The new type of dilute magnetic semiconductor(Y_(0.75)Ca_(0.25))(Cu_(0.75)Mn_(0.25))SO exhibits significant light loss around 70 eV,with light reflection gradually increasing after 30 eV,and light absorption mainly occurring around 8-30 eV.These results also provide a basis for the discovery of more types of 1111 phase new dilute magnetic semiconductors in the future.

Effect of CO_(2) dilution on laminar burning velocities,combustion characteristics and NO_(x) emissions of CH_(4)/air mixtures

The laminar combustion characteristics of CH_(4)/air premixed flames with CO_(2) addition are systemically studied.Experimental measurements and numerical simulations of the laminar burning velocity(LBV)are performed in CH_(4)/CO_(2)/Air flames with various CO_(2) doping ratio under equivalence ratios of 1.0–1.4.GRI 3.0 mech and Aramco mech are employed for predicting LBV,adiabatic flame temperature(AFT),important intermediate radicals(CH_(3),H,OH,O)and NO_(x) emissions(NO,NO_(2),N2O),as well as the sensitivity analysis is also conducted.The detail analysis of experiment and simulation reveals that as the CO_(2) addition increases from 0%to 40%,the LBVs and AFTs decrease monotonously.Under the same CO_(2) doping ratio,the LBVs and AFTs increase first and then decrease with the increase of equivalence ratio,and the maximum of LBV is reached at equivalence ratio of 1.05.The mole fraction tendency of important intermediates and NO_(x) with equivalence ratio and CO_(2) doping ratio are similar to the LBVs and AFTs.Reaction H+O_(2)⇔O+OH is found to be responsible for the promotion of the generation of important intermediates and NO_(x) under the equivalence ratios and CO_(2) addition through sensitivity analysis.The sensitivity coefficients of elementary reactions that the increasing of CO_(2) doping ratio promotes or inhibits formation of intermediate radicals and NO_(x) decreases.

Dilution characteristics of dual buoyant jets in wavy cross-flow environment

Due to the difference in density between the discharge effluent and coastal water,partially treated wastewater is often discharged into the marine environment as a buoyant jet via submarine outfalls with multiport diffusers.The dilution characteristics of effluent discharge(dual buoyant jets)in a wavy cross-flow environment were studied in a laboratory.The planar laser-induced fluorescence technique was used to obtain the concentration data of the jets.The effects of different environmental variables on the diffusion and dilution characteristics of the jets were examined through physical experiments,dimensional analysis,and empirical formulations.It was found that the dilution process of the dual jets could be divided into two components:the original jet component and the effluent cloud component.The jet-to-current velocity ratio was the main parameter affecting the concentration levels of the effluent cloud.The merging of the two jets increased the jet concentration in the flow field.When the jets traveled further downstream,the axial dilution increased gradually and then increased significantly along the axis.Under the effects of strong waves,the concentration contours branched into two peaks,and the mean dilution became more significant than under the effects of weak waves.Therefore,the dilution of the effluent discharge was expected to be significant under strong wave effects because the hydrodynamic force increased.A dilution equation was derived to improve our understanding of the dilution process of buoyant jets in a wavy cross-flow environment.This equation was used to determine the influences of the jet-to-current velocity ratio,wave-to-current velocity ratio,and Strouhal number on the minimum jet dilution.It revealed that the wave and buoyancy effects in effluent discharges were significant.

What Is the Difference between Post- and Pre-Dilution in On-Line Haemodiafiltration in the Removing of Median-Molecular-Weight Toxins?

Introduction: β2-microglobulin and prolactin are medium-molecular-weight toxins. We believe that the rate of removal of these molecules, using filters with two different surfaces, in post- and pre-dilution haemodiafiltration, will be of interest to the literature. Methods: We studied, in 12 haemodialyzed patients, the removal of those, with filter with surface of 2.5 m2 (Group A) or 2.1 m2 (Group B) with post-dilution haemodiafiltration, and with a filter with surface 2.5 m2 with pre-dilution (Group C). Results: Satisfactory removal of β2-microglobulin (best with post-dilution) was found, and a good rate of removal of prolactin without the filter surface played a role in both cases. Conclusion: The elimination of β2-microglobulin in post-dilution is not affected by the filter surface area. Pre-dilution achieves removal of β2-microglobulin, less than that of post-dilution. Prolactin was removed satisfactorily regardless of the filter surface in post-dilution, and its removal appears to be less than that of β2-microglobulin.

铜渣贫化回收铜的研究现状及展望

铜是现代工业不可或缺的原材料,然而我国铜资源对外依存度高,是典型的“卡脖子”资源。铜主要通过火法冶炼铜精矿制得,冶炼过程渣量大、渣含铜量高达0.5%~5%,远高于我国铜矿的可采品位(0.2%)。因此,研究铜渣贫化回收铜的工艺对提升我国资源保障能力具有重要意义。基于铜/铜锍在渣中的赋存状态、铜损的主要形式,重点综述了现阶段铜渣贫化回收铜的工艺技术,包括火法贫化法、浮选法、湿法处理等,并对未来的研究重点进行了展望。目前,电炉贫化处理量大,技术成熟,但其通常使用煤炭等作为还原剂,由于其密度小于铜渣,反应时大多漂浮渣层表面并燃烧,反应不充分,也不利于大气环保。另外,工业上常使用金属铁棒还原炉底结瘤的磁铁矿,但其密度大于铜/铜锍,在渣液中沉降速度快,对渣层的还原不彻底。因此,开发环保、高效的还原剂逐渐成为火法电炉贫化研究的重点。浮选法是处理天然铜矿的常用手段,但铜渣存在硬度高、伴生关系复杂、粒度分布不均、微细粒多等浮选难点,同时铜渣高温浮选导致捕收剂失活的问题也亟待解决。在处理低品位铜渣时,湿法浸出是常用手段,但化学试剂和废液环保问题难以解决;生物浸出具有性质稳定、对环境无污染,且浸出后金属含量较低等优点,但其浸出周期长、效率低。根据目前贫化工艺的难点,对未来贫化工艺开发与优化进行了展望,如增加外场聚集四氧化三铁以改善铜/铜锍沉降环境、开发环保高效的火法贫化还原剂、探究还原剂对不同铜渣渣型的作用机制以及开发耐高温的铜渣浮选新药剂等。

基于组合圆锥构型的水下声学定位系统布站优化

在水下目标定位中,布站构型的共面约束会导致目标单点定位的几何精度因子(GDOP)理论最小值不能达到。为改善水下布站的观测矩阵,将单圆锥扩展为组合圆锥构型布站模式。然而,传统的优化算法易陷入局部最优且存在收敛效率低等问题。针对以上问题,提出了一种改进的自适应粒子群算法。首先提出了一种有共面约束的水下声学定位系统组合圆锥构型,并证明了所提出的组合圆锥构型具有可叠加性、可旋转性以及GDOP旋转不变性;其次,针对布站优化指标单一的问题,构建了一种基于水下目标全局GDOP的布站优化准则;在此基础上提出了一种基于自适应粒子群的优化算法,并应用于组合圆锥构型下的水下声学定位系统布站优化。所提出的自适应粒子群算法能增强布站的全局最优性,提高算法收敛效率和水下目标的定位精度。

基于CFD-DEM算法的气力输送气固两相流特性分析

超轻粉体颗粒由于质量较小,在运输过程中易受气流扰动而飘散,物料的管道气力输送过程不稳定,易发生堵塞。为了研究超轻粉体颗粒在旋流气力输送中气固两相流流动特性,采用计算流体力学与离散单元法(CFD-DEM),对Komax型静态混合器内气固两相流动特性进行数值模拟研究。研究发现,带有Komax型元件的水平管道可以改变颗粒的流动情况,改善了水平管道内颗粒堆积和分布不均匀的现象;分别从颗粒相和流体相的流动状态分析得到元件长径比Ar=3时为最优几何结构;通过正交实验极差分析得到影响气固两相流动特性的因素顺序:输送气速>颗粒质量流量>颗粒粒径。当元件Ar=3时,颗粒-颗粒和颗粒-管壁的碰撞次数与碰撞强度呈现负相关,结合出口颗粒流分散状态,优选输送气速为3~4m/s;主要考虑输送气速对管内压降的影响,提出了带有Komax型元件的水平管道气力运输过程中压降与输送气速和轴向位置的经验拟合式。

肉桂精油复配香芹酚和百里香酚对食用畜禽有害微生物熏蒸的抗菌活性

通过测定抑菌圈直径确定肉桂精油及单离香料香芹酚和百里酚对食用畜禽有害微生物的敏感性,同时采用气相熏蒸法测定最低抑菌浓度(Minimum Inhibitory Concentration,MIC)和最低杀菌浓度(Minimum Bacterial Concentration,MBC)。结果表明:肉桂精油及香芹酚和百里酚对食用畜禽有害微生物都具有一定的抑杀能力。肉桂精油对黑曲霉的抗菌效果优于百里香酚和香芹酚,肉桂精油对黑曲霉的MIC和MBC为62.5μL/L,而百里香酚和香芹酚的MIC和MBC均为125μL/L;将肉桂精油与香芹酚进行复配,复配精油对白色葡萄球菌和黑曲霉均表现出相加作用(FICI≤1),而对白色念珠菌则表现为无关作用。通过GC-MS分析,肉桂精油的主要挥发性化学成分中相对含量较高的为肉桂醛(78.19%)、2-甲氧基肉桂醛(8.70%)。采用电子鼻分析溶剂稀释后对复配精油抑菌活性的影响,抑菌能力大小为:丙二醇稀释≈无水乙醇稀释>未稀释>甘油稀释>食用油稀释。实验表明:香芹酚与肉桂精油复配可以提高肉桂精油的抗菌活性,溶剂挥发性的差异会对复配精油的抑菌活性造成不同影响,稀释复配精油时溶剂的较优选择为丙二醇。

裂解炉稀释蒸汽管道三通开裂原因分析

针对某乙烯裂解装置稀释蒸汽管道304H耐热不锈钢三通使用1年后发生开裂的情况,从材料成分、力学性能、金相组织、残余应力和断口特性等方面进行了分析。结果表明,裂纹分别启裂于三通的内壁和外壁,多数裂纹开裂处伴有晶间腐蚀特征,裂纹扩展特性以沿晶型为主;断口附近腐蚀产物存在O,S,Cl等酸性腐蚀介质。三通主管表面最大轴向应力达到147 MPa,三通相贯线附近距裂纹20 mm处的最大环向应力达到114 MPa,说明运行中的三通表面应力达到了材料屈服强度的1/2。分析认为,裂纹的产生是由于材料发生敏化后,在应力和腐蚀介质共同作用下形成的以沿晶为主的应力腐蚀开裂,更换三通材料或通过适当的固溶处理降低三通中的残余应力是避免三通开裂的重要途径。

直接稀释-电感耦合等离子体质谱法测定母乳中17种元素的含量

提出了直接稀释-电感耦合等离子体质谱法(ICP-MS)同时测定母乳中钒、铬、锰、钴、镍、铜、锌、砷、硒、锶、钡、钼、镉、锡、锑、汞、铅等17种元素含量的方法。取母乳0.5 mL,用含2%(体积分数)硝酸和0.01%(体积分数)四甲基氢氧化铵的0.01%(体积分数)曲拉通X-100溶液定容至10 mL,涡旋混匀,以转速4000 r·min^(-1)离心5 min,将上清液用0.45μm水相滤膜过滤,在动能歧视(KED)模式下采用ICP-MS测定滤液中上述17种元素的含量,在线加入含6μg·L^(-1)钪、锗、铑、铋的混合内标使用液。结果表明:各元素的质量浓度在一定范围内与所对应的信号强度与内标元素信号强度比呈线性关系,检出限(3s)为0.019~0.768μg·L^(-1);方法用于分析美国国家标准参考材料,除锌元素外,其他元素的测定值均在认定值的不确定度范围内,并且日内和日间的变异系数均小于13%;按照标准加入法进行回收试验,回收率为81.3%~119%。

MILD粉体燃烧技术研究进展与关键问题分析

MILD燃烧是一种在中度或极度低氧环境下发生的温和燃烧模式,兼具高燃烧热利用率和极低NOx排放的优势,国际燃烧领域认为它是拥有巨大应用潜力的清洁燃烧技术之一。自1990年左右开展相关研究以来,对于实现气体燃料的MILD燃烧的相关技术已相对成熟,而关于煤粉和生物质等固体燃料的MILD燃烧机制和实现条件的研究仍相对缺乏。基于高动量氧化剂射流来实现内部再循环,不再需要外部高温预热来建立MILD燃烧,极大拓宽了MILD燃烧的应用范围。从颗粒弥散、受热、着火、燃烧、污染物等方面概述了MILD粉体燃料燃烧的基础特性,由于颗粒的不均匀弥散和反应,煤粉等碳基固体燃料的MILD燃烧进程较气体燃料更复杂。高速射流MILD燃烧在增加点火延迟的同时也扩展了点火区和反应区,需要对燃烧各阶段的特征和机理开展系统研究。介绍了固体燃料MILD燃烧理论设计和装备研发领域所取得的研究成果,建议通过高精度数值模拟,改进现有燃煤锅炉燃烧器、调节工艺参数以匹配MILD燃烧模式,增加焦炭颗粒的停留时间以提高燃烬率,提高燃烧稳定性并抑制包括细颗粒物在内的各类污染物排放。基于互联能源系统的整体方法,推进MILD燃烧与各类新型燃烧技术的耦合研究,尤其加强煤粉、生物质与氢、氨等可燃气体共燃特性研究,助力能源转型。探究粉体MILD燃烧中的湍流两相流特征、湍流相间传热作用以及湍流-化学耦合作用是加深对粉体MILD燃烧理解的关键,涉及多变量分析和高精度模拟,是未来研究的重点和难点。

波流共同作用下射流稀释特性的动量积分模拟研究

污水通常以射流的形式向海排放,其在海洋环境水体中的稀释过程是射流与波浪、潮流共同作用的结果。本文基于合理的假设条件,对射流运动的控制方程进行积分处理,结合波流环境下射流的结构特征,引入射流卷吸与拖曳力函数,结合必要的边界条件,形成封闭的控制方程组,建立波流环境下射流动量积分模型。通过与实验资料的对比分析可以看出,该模型可以准确模拟波流环境下射流在近区段的时均运动与稀释过程;相较于单一的横流作用,波流共同作用下射流对周边水体的影响范围更大,射流初始稀释能力更强。基于多个组次的动量积分模拟实验,通过无量纲分析与最小二乘拟合,建立了波流共同作用下射流轨迹中心线位置及最小稀释度的经验公式。相关成果可为排海污水环境影响评估提供快速、准确的分析手段。

不同氮效率春玉米品种临界氮浓度稀释曲线建立与验证

采用田间定位试验,以山西省晋中地区春玉米各生育时期地上部干物质量与植株氮浓度的变化规律,建立春玉米临界氮浓度稀释曲线模型,为实现春玉米绿色增产与氮素管理提供理论依据。本研究以玉米品种‘郑单958’和‘大丰26’为试验材料,设4个施氮量处理:0 kg(N)∙hm^(−2)(N0)、120 kg(N)∙hm^(−2)(N120)、240 kg(N)∙hm^(−2)(N240)和360 kg(N)∙hm^(−2)(N360),于2014—2016年在山西农业大学东阳试验基地开展3年定位施氮试验,在春玉米拔节期(V6)、抽雄期(VT)、灌浆期(R2)和成熟期(R6)采集植株样品,分析两个春玉米品种在不同施氮量处理下地上部干物质量、籽粒产量(以下简称“产量”)和各生育时期植株氮浓度,以不同生育时期干物质累积量和植株氮浓度,建立并验证两个春玉米品种的临界氮浓度稀释曲线模型。结果表明,‘郑单958’氮素利用率高于‘大丰26’。两个春玉米品种在适宜施氮量条件下,各生育时期地上部干物质量和产量均随施氮量增加呈增加趋势,地上部干物质量在N240和N360处理间差异不显著,产量在N240处理达最大值;植物氮浓度随施氮量增加而增加,随春玉米生育进程推进与地上部干物质量呈幂指数关系。依据春玉米地上部干物质量(Md)与其对应的植株氮浓度(CN)变化关系,建立两个春玉米品种的临界氮浓度稀释曲线模型:‘郑单958’CN=30.457Md−0.292,‘大丰26’CN=33.249Md−0.333。相比‘大丰26’的模型参数,‘郑单958’的模型参数a降低8.40%,参数b降低12.31%;‘郑单958’和‘大丰26’模型均方根误差(RMSE)分别为1.71 g∙kg^(−1)和1.54 g∙kg^(−1),标准化均方根误差(n-RMSE)分别为9.25%和8.27%,表明模型稳定性较好。氮营养指数在同一生育时期随施氮量增加呈上升趋势,随生育时期推进呈先增加后降低趋势,与各生育时期的相对干物质量呈显著线性相关,与相对产量呈显著的一元二次曲线关系。本研究建立的晋中地区两个春玉米品种临界氮浓度稀释曲线模型及各生育时期氮营养指数,可用于春玉米生育时期营养状况的诊断和评估,结合施氮量与产量的关系,推荐该试验区域‘郑单958’施氮量为189.16~224.08 kg∙hm^(−2),‘大丰26’施氮量为199.72~214.67 kg∙hm^(−2)。

2022年8月北黄海北部溶解甲烷分布、海-气交换通量及影响因素

科学评估陆架边缘海溶解甲烷(CH_(4))的分布及海-气交换通量对于认识陆架边缘海CH_(4)的释放对大气CH_(4)的区域性贡献具有重要意义。基于2022年8月的现场调查数据和资料,研究北黄海北部海水溶解CH_(4)的分布、海-气交换通量及影响因素。结果表明:研究海域溶解CH_(4)浓度为4.0~63.3 nmol/L,饱和度为168%~2 360%,高值区位于鸭绿江口附近海域,随着离岸距离的增加表层海水溶解CH_(4)浓度迅速降低。鸭绿江等陆源冲淡水的输入耦合海水及沉积物有机质的降解致使近岸海域海水CH_(4)升高;陆源冲淡水与海水混合过程中海水CH_(4)的氧化消耗也是控制CH_(4)浓度和分布不容忽视的重要过程。离岸海域海水及沉积物有机质厌氧降解耦合黄海冷水团的作用使得底层海水溶解CH_(4)浓度高于表层海水。研究海域海-气CH_(4)交换通量为18.4~578.8μmol/(m^(2)·d),是大气CH_(4)的源;鸭绿江口附近海域海-气CH_(4)交换通量高于离岸海域。由此可见,受陆源冲淡水输入的影响研究海域溶解CH_(4)浓度和海-气交换通量具有显著的区域性差异,且变幅高于世界其他海域;加强河口以及近海调查研究对于准确评估陆架边缘海CH_(4)的排放,明确CH_(4)排放源项的构成及制定CH_(4)减排的有效措施至关重要。

分离多环芳烃用于超稠油掺稀降黏的研究

针对炼油厂催化裂化柴油大量过剩和芳烃含量过高等问题,结合稠油掺稀降黏开采掺稀比高、稀油资源紧缺的现状,从催化裂化柴油中萃取分离多环芳烃,用于超稠油掺稀降黏研究。对多环芳烃萃取进行正交试验,在筛选出的最佳操作条件(萃取温度为45℃、萃取时间为5 min、相分离时间为5.5 min和剂油体积比为1.4)下,多环芳烃产品收率为29.87%、芳烃质量分数高达99.07%。在掺稀比均为0.10时,多环芳烃和塔河稀油的掺稀降黏量率分别为94.20%和68.58%。拟合计算结果表明,多环芳烃用量仅为塔河稀油的16.32%时,即可达到塔河油田稠油掺稀降黏要求。以塔河油田稠油自喷井为例,当稠油含水率分别为0,30%和50%时,掺入多环芳烃相对掺入稀油的单井日产油增长率分别达到115.90%,84.57%,62.20%。

超低稀释比熔融制样X射线荧光光谱法测定铀矿石中主次量元素

铀矿属于国家战略性矿产,目前对铀矿石的分析以化学法为主,方法成熟,标准化程度高,但操作复杂,步骤繁琐。而采用X射线荧光光谱法进行分析,样品用量大,无法用于极少量样品分析。选用四硼酸锂和偏硼酸锂混合熔剂,与样品以100∶1的超低稀释比熔融制样,利用波长色散X射线荧光光谱法测定铀矿石中Si、Al、Fe、Ca、Mg、K和U等元素。采用多个铀矿石标准物质和人工配制的工作标准制作标准曲线,理论α系数及康普顿散射内标法校正元素间的吸收增强效应,讨论了样片厚度对于样品测量的影响。方法精密度(RSD,n=10)介于0.7%~3.4%之间,且U元素方法检出限可低至15μg·g^(-1)。采用未参加回归的标准物质验证方法准确度,测量结果均在不确定度范围内。本方法通过选择有效的助熔剂和极低的稀释比,解决了X射线荧光法样品用量大,无法分析极少量样品的问题。

基于不确定度评估研究ID-LC-MS/MS法检测鸡蛋中氟虫腈砜残留量的关键控制点

为了控制检测结果准确性,以鸡蛋粉中氟虫腈砜残留分析标准物质[GBW(E)100779]为测试样,采用“自下而上”法对基于多功能净化柱(PAC柱)净化的同位素稀释液相色谱串联质谱(ID-LC-MS/MS)法进行测量不确定度评估。“鱼骨图”分析表明,不确定度分量主要来源有样品称样量、内标溶液添加体积、标准工作溶液浓度及其移取体积。内标溶液添加体积引入的不确定度最大,对检测结果不确定度的贡献率为68.59%;万分之一天平称量引入的不确定度可忽略不计。同位素内标的添加过程是ID-LC-MS/MS法检测的关键控制点,参考基准的合理选择和目标物的完全提取是准确测量的前提。进一步用LC-MS/MS法对参考物质、稀释剂和内标溶液的适用性进行了评估,并基于国家有证标准物质[GBW(E)100779]对提取方法进行了优化。研究结果有利于提升鸡蛋食品安全的检测质量和质控水平,为精准检测质控方案的设计提供新思路。